The effects of composition, temperature and hydrostatic pressure on phase transition behaviors in (Pb1-1.5xLax)(Zr0.8Ti0.2)O3 ceramics

The effects of composition, temperature and hydrostatic pressure on phase transition behaviors in (Pb1-1.5xLax)(Zr0.8Ti0.2)O3 ceramics | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article The effects of composition, temperature and hydrostatic pressure on phase transition behaviors in (Pb 1-1.5x La x )(Zr 0.8 Ti 0.2 )O 3 ceramics Meng Xie, Yizheng Bao, Hengchang Nie, Fei Cao, Xianlin Dong, Genshui Wang This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-25916/v1 This work is licensed under a CC BY 4.0 License Status: Posted Version 1 posted You are reading this latest preprint version Abstract In this work, (Pb 1 − 1.5 x La x )(Zr 0.80 Ti 0.20 )O 3 (abbreviated as PLZT, x = 0.01, 0.03, 0.04, 0.06, 0.07) ceramics are designed on the base of chemical composition modification and prepared by solid-state reaction. The effect of composition, temperature, and hydrostatic pressure on ferroelectric-antiferroelectric (FE-AFE) phase transition is investigated. It is obtained that phase transition from ferroelectric rhombohedral phase to antiferroelectric tetragonal phase as a function of La 3+ doping content, especially, the PLZT ceramics of x = 0.04, 0.06, and 0.07 are the coexistence of FE-AFE phase. It is also found the FE-AFE phase transition driven by increased temperature in poled PLZT ceramics ( x = 0.04, 0.06). Furthermore, static charges density ( P r ) of PLZT ( x = 0.04, 0.06) are decreased from 29.11 µC/cm 2 and 31.52 µC/cm 2 to 19.76 {\mu }C/cm 2 , 6.45 {\mu }C/cm 2 under 400 MPa hydrostatic pressure due to the pressure-induced FE-AFE phase transition. The depolarization rates are 32.12% and 79.54%, respectively. Meanwhile, the phase diagram of (Pb 1 − 1.5 x La x )(Zr 0.80 Ti 0.20 )O 3 ceramics is acquired roughly. These results provide guidance for the engineering application of (Pb 1 − 1.5 x La x )(Zr 0.80 Ti 0.20 )O 3 ceramics. Ceramics Phase transition PLZT ferroelectrics anti-ferroelectrics Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 1. Introduction Ferroelectric (FE) lead-containing materials with spontaneous polarization, is the significant functional materials and has been studied for many years [1]. Lead zirconate titanate (Pb(Zr,Ti)O 3 , (PZT)) ceramics with outstanding piezoelectric and ferroelectric properties are representative compositional system for ferroelectric materials, widely utilized in modern ferroelectric transducers, sensor, actuators and ultrahigh-power system [2–6]. Based on reported studies, modification with dopants has been an acknowledged and effective approach to optimize the performance of PZT ceramics [7–12]. In particular, compositions near phase boundary have been concentrated on more interest over the past few decades, because of that phase transition of polar state and nonpolar state involving to the generation/release electric polarization have a wide range of applications [7, 13–15]. Pb(Zr,Sn,Ti)O 3 , (Pb,Nb)(Zr,Sn,Ti)O 3 , and (Pb,La)(Zr,Sn,Ti)O 3 ceramics obtained through modification of PZT ceramics with Sn and La are all promising ferroelectric materials, extensively studied and applied [7, 8, 16]. In addition, (Pb,La)(Zr,Ti)O 3 (PLZT) ceramics acquired through modification of PZT ceramics with lanthanum (La) are also representative ferroelectric materials [17–22]. The coupling of ferroelectric reactive oxygen octahedrons broken by the replacement of La 3+ (1.36 Å) for Pb 2+ (1.49 Å) at A-sites give rise to phase transformation[19, 23]. In particular, the excellent piezoelectricity, pyroelectricity and energy-storage properties are possessed by compositions located in phased boundary [19, 24–28]. For example, Ciuchi et al. investigated the energy storage performances of (Pb 1 − x La x )(Zr 0.90 Ti 0.10 ) 1− x /4 O 3 ceramics with La compositions near the FE-AFE phase boundary [26]. Qiao et al. reported the effect of FE-AFE phase transition on enhanced pyroelectric properties in (Pb 1 − 1.5 x La x ) (Zr 0.86 Ti 0.14 ) O 3 ceramics [27]. Besides, high piezoelectricity of PLZT ceramics near phase boundary was evident by Kumar et al [28]. In general, it’s fundamental and significant to investigate the phase transition in PLZT ceramics for application. However, to date, there were rare attentions paid to the effect of composition, temperature, especially, hydrostatic pressure on FE-AFE phase transition in (Pb 1 − 1.5 x La x ) (Zr 0.80 Ti 0.20 ) O 3 . In this paper, the effect of composition, temperature, and hydrostatic pressure on phase transition behaviors in (Pb 1 − 1.5 x La x ) (Zr 0.80 Ti 0.20 )O 3 ( x = 0.01, 0.03, 0.04, 0.06, 0.07) ceramics are investigated thoroughly. XRD patterns, temperature-dependent P-E hysteresis loops, and temperature-dependent dielectric constant curve demonstrate phase transition between FE R and AFE T driven by increased La content and temperature. What’s more, the depolarization behaviors of poled PLZT( x = 0.04, 0.06) under hydrostatic pressure are investigated. These results indicate La doping at A-sites reconfigures the phase boundary of FE state and AFE state in PLZT ceramics. Besides, it also unveil the FE-AFE phase transition of (Pb 1 − 1.5 x La x )(Zr 0.80 Ti 0.20 )O 3 ceramics for promising potential engineering applications. 2. Experimental Procedure (Pb 1 − 1.5 x La x )(Zr 0.8 Ti 0.2 )O 3 ( x = 0.01, 0.03, 0.04, 0.06, 0.07) ceramics were prepared via conventional solid reaction method. Raw materials were reagent-grade metal oxides Pb 3 O 4 (99.5%), La 2 O 3 (99.95%), ZrO 2 (99.99%), TiO 2 (99.21%). 0.5 mol% additional Pb 3 O 4 were added in order to compensate Pb volatilization during sintering. The powders were weighted according to the stoichiometric composition and ball milled 12 h in Teflon jars with deionized water and zirconium ball as media. After drying, the powders were calcined at 925 \text{℃} for 2 h. And the calcined powders were ball milled again for 24 h. The polyvinyl alcohol (PVA), a binder for granulation, was mixed into calcined powders. The powders were pressed into pellets with 13 mm diameter. After burning off PVA, the pellets buried with same composition to minimize Pb volatilization in alumina crucible, were sintered at 1300 \text{℃} for 2 h with a heating rate of 2 \text{℃} /min. The sintered pellets were polished to a thickness of 0.5 mm and both sides of samples were covered with fired-on silver paste, calcined at 600 \text{℃} for 2 h. Crystal structure was studied by using X-ray diffraction (XRD, D/MAX-2550V; Rigaku, Tokyo, Japan). Cross-sectional microstructure was observed using a TM 3000 Tabletop Microscope (Hitachi, Tokyo, Japan). The dielectric constant ( {\epsilon }_{r} ) and tangent loss ( tan\delta ) were tested by using a LCR meter (Model E4980; Agilent, Palo Alto, CA, USA). Polarization-electric field ( P-E ) hysteresis loops and depolarization behaviors under hydrostatic pressure were measured using an aixACCT TF 2000 Analyzer FE measuring by system (aix ACCT Co., Aachen, Germany) with home-made hydrostatic loading apparatus [29]. 3. Result And Discussion 3.1 Structure properties As shown in Fig. 1 , the perovskite structure with second phases PbO 2 (PDF#50-1430) is observed in the XRD patterns of PLZT ceramics. The peak is shifted slightly to higher 2 {\theta } with the increased La content, indicating decrease of lattice constant and smaller unit cell volume, attributed to oxygen octahedral distortion causing by the replacement of La 3+ (1.36 Å) for Pb 2+ (1.49 Å) at A-sites. Detailed XRD patterns in 2 {\theta } plotted in Fig. 1 b and Fig. 1 c, it can be observed the peak splitting in the (111) reflections in the PLZT ceramics of x = 0.01, 0.03, indicating a predominantly rhombohedral distortion, that is, the nature of FE R phase. With increased La content ( x = 0.04, 0.06, 0.07), the peak splitting are observed in the (200) reflections and the (111) reflections are gradually transformed to single peak, indicating the phase switching to tetragonal distortion, that is, the coexistence of FE R phase and AFE T phase [30]. The result reveals that the occurrence of FE R -AFE T phase transition is driven by increased La content. The cross-sectional SEM images of fresh samples sintered at 1300 °C are shown in Fig. 2 . With increased La content, the grain size is decreased significantly. In addition, these cross-sections are fractured along intergranular direction under external force when La content x = 0.01, 0.03 and 0.04; whereas cross-sections for x = 0.06 and 0.07 are fractured along trans-granular direction under external force. 3.2 Dielectric properties Temperature-dependent relative dielectric constant ( {\epsilon }_{r} ) and dielectric loss ( tan\delta ) of PLZT ceramics as a function of temperature at different frequencies are displayed in Fig. 3 a-e. Similar temperature-dependent behavior at the Curie temperature {(T}_{C}) are obsevered in the samples of x = 0.01 and 0.03. T C is defined by the temperature of the maximum dielectric constent, regarded as a thermodynamic scale for the transition energy barrier from the FE or AFE phase to paraelectric (PE) phase. [31] While two dielectric anomalies can be observed in the PLZT ceramics of x = 0.04 and 0.06: T FE−AFE and T C . T FE−AFE can be determined by the first dielectric constant inflection point and dielectric loss peak, attributed to the transformation from FE to AFE. Hence, T FE−AFE has also been regared as the depolarization temperature ( T d ) of the sample. As for the sample with x = 0.07, it can be only seen phase transition from AFE to PE since the AFE phase is dominanted. In Fig. 3 f, the T C corresponding to the samples of x = 0.01, 0.03, 0.04, 0.06, 0.07 are 240 \text{℃} , 207 \text{℃} , 143 \text{℃} , 128 \text{℃} , 114 \text{℃} , respectively. Furthermore, \epsilon max is decreased from 42025 to 5435 with increased La content, and the tan\delta is less than 0.083. Therefore, it is confirmed that the PLZT ceramics of x = 0.04, 0.06 are lying around the FE-AFE phase boundaries and experience FE-AFE phase transition near 125 \text{℃} and 80 \text{℃} , while the PLZT ceramics of x = 0.01, 0.03 are stable FE R before T C . 3.3 Ferroelectric properties The P-E hysteresis loops of all as-sintered specimens from 30 \text{℃} to 170 \text{℃} can be observed in Fig. 4 to further confirmed temperature-induced phase transition shown in Fig. 3 . As shown in Fig. 4 a, b, well-shaped P-E hysteresis loops show that these components are stable FE R independent of temperature, where 170 \text{℃} is less than T C shown in Fig. 3 a and b. PLZT ceramics of x = 0.04, 0.06 are transformed from well-shaped P-E loops to double hysteresis loops and then to slim P-E loops, indicating transition of FE phase to AFE phase and then to PE phase [32, 33]. Phase transformation from AFE to PE with La content x = 0.07 is exhibited in Fig. 4 e. Moreover, the phase transition temperature is decreased from about 130 \text{℃} to 90 \text{℃} with increased La content corresponding to Fig. 3 f, in which defects produced by the aliovalent substitution and the long range order of ferroelectric domains destroyed are beneficial to the inversion of domain wall [34]. P r and coercive field E C are decreased remarkably and the loops are much slimmer with further increased temperature and La content [1]. In the Fig. 4 f and Fig. 3 f, it can be observed excellent temperature stability for P r of samples of x = 0.01, 0.03; while there is a sharp decrease in P r for samples of x = 0.04, 0.06, proving temperature dominates FE-AFE transition. In a way, there is temperature-induced structural phase transition and depolarization behaviors in the PLZT ceramics of x = 0.04 and 0.06. 3.4 Depolarization under hydrostatic pressure PLZT( x = 0.04, 0.06) ceramics with higher P r and near the phase boundary between FE and AFE phase are chosen to study the depolarization under hydrostatic pressure. These samples were polarized at 2.0 kV/mm for 15 min at room temperature in an silicone oil bath, and then placed for 24 h after polarization to obtain stable P r . P-E hysteresis loops and I-E loops of PLZT( x = 0.04, 0.06) ceramics at electric field of 4 kV/mm and under the hydrostatic pressure increasing from 0 MPa to 400 MPa are shown in Fig. 5 . Well-shaped P-E hysteresis loops with the P r decreased from 29.11 µC/cm 2 to 19.76 µC/cm 2 are shown in Fig. 5 (a1). It’s also observed that the maximum pressure used in the experiment do not reach the critical depolarization pressure. What’s more, E C is decreased from 1.09 to 0.94 kV/mm with increased pressure to 400 MPa, indicating that a predominant FE ordering gradually decreases. As shown in Fig. 5 ( a2), with increased hydrostatic pressure, the current peak gradually slows down and the polarization is gradually released in the form of current under additional field. Clearly, the P r of sample x = 0.06 is decreased from 31.52 {\mu } C/cm 2 to 6.45 {\mu } C/cm 2 , as shown in the Fig. 5 (b1). It’s exhibited in Fig. 5 ( b2) that the single current peak is transformed to double current peak with the transition from FE R phase to AFE T phase under the effect of hydrostatic pressure, which is similar to temperature-induced phase transition shown in Fig. 3 and Fig. 4 . According to soft mode theory, hydrostatic pressure with spherical symmetry increases the interactions between adjacent cations and anions more rapidly than it increases long-range Coulomb forces, increasing the AFE phase stability, and releasing stored charges in a very short period of time [30]. To further evaluate pressure-induced depolarization behaviors, the remnant polarization of poled PLZT ( x = 0.04, 0.06) are shown in Fig. 6 (a). It can be observed that the P r of x = 0.04 is decreased steadily under hydrostatic pressure, and the P r of x = 0.06 is decreased rapidly after hydrostatic pressure of 250 MPa. Meanwhile, the remnant polarizations are decreased from P r1 = 29.11 µC/cm 2 , 31.52 µC/cm 2 to P r2 = 19.76 µC/cm 2 , 6.45 µC/cm 2 , respectively, with depolarization rates of 32.12% and 79.54%,calculated by (see Equation 1 in the Supplementary Files) {R}_{T}=-\frac{{P}_{r2}-{P}_{r1}}{{P}_{r1}}\times 100\% under 400 MPa pressure. These results demonstrate that the oriented FE domains are rearranged under the influence of hydrostatic pressure, accompanied by irreversible FE-AFE phase transition and the release of polarization. The results also demonstrate the promising potential application of (Pb 1−1.5 x La x )(Zr 0.8 Ti 0.2 )O 3 ceramics in pulsed power supply. Based on the above results, a simple phase diagram of (Pb 1 − 1.5 x La x )(Zr 0.8 Ti 0.2 )O 3 ceramics is proposed. The phase diagram of PLZT ceramics for x = 0.01, 0.03, 0.04, 0.06, 0.07 are summarized in Fig. 6 (b), determined by the temperature of T C corresponding to the maximum values of dielectric constant and dielectric loss in the Fig. 3 , employed to classify the boundary of FE and PE phase. The AFE phase can be stabilized by doping La 3+ and destabilized by Ti 4+ doping [5], so that PLZT ceramics are transformed from FE to AFE phase with La doping, manifesting AFE phase tends to be stable and a FE-AFE phase boundary is constructed by La in PLZT-based ceramics [35, 36]. 4. Conclusion In summary, the effect of composition, temperature and hydrostatic pressure on phase transition behaviors in (Pb 1 − 1.5 x La x )(Zr 0.80 Ti 0.20 )O 3 ceramics were investigated thoroughly, with emphasis on ferroelectric, dielectric performances, and depolarization behaviors. With increased La content, PLZT ( x = 0.01, 0.03, 0.04, 0.06, 0.07) ceramics underwent transition from FE R phase to AFE T phase. Aliovalent A-site substitution of La 3+ doping interrupted long-range ordered ferroelectric domains, driving FE R -AFE T phase switching. The lattice constant was decreased and the peak value was shifted to higher 2 {\theta } as a whole. Temperature-dependent P-E hysteresis loops and temperature-dependent relative dielectric constant ( {\epsilon }_{r} ) and dielectric loss ( tan\delta ) demonstrated PLZT( x = 0.01, 0.03) ceramics were stable FE R phase, while PLZT( x = 0.04, 0.06, 0.07) coexisted FE phase and AFE phase. With the increase of temperature, the domains overcame the energy barrier to achieve FE-AFE phase transition. There was thermal-induced FE-AFE phase transition and depolarization behaviors in the PLZT ceramics of x = 0.04, 0.06. Pressure-dependent P-E loops and I-E loops illustrated the polarized sample PLZT ( x = 0.04, 0.06) ceramic could be depolarized with depolarization rate of 38.51% and 79.54%, respectively. According to the effect of external field on FE-AFE phase transition, it indicated that (Pb 1 − 1.5 x La x )(Zr 0.8 Ti 0.2 )O 3 ceramics had promising potential in the field engineering application. 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[36] Peng P, Nie H, Cheng G, et al. Thermal-induced structural transition and depolarization behavior in (Bi 0.5 Na 0.5 )TiO 3 -BiAlO 3 ceramics. J Appl Phys 2018, 123 : 114102. Supplementary Files Equation1.pdf Cite Share Download PDF Status: Posted Version 1 posted You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. We do this by developing innovative software and high quality services for the global research community. Our growing team is made up of researchers and industry professionals working together to solve the most critical problems facing scientific publishing. Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-25916","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":533371,"identity":"0ef78d64-9f14-4bd5-adf9-438c070dabee","order_by":1,"name":"Meng Xie","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAABGElEQVRIie2PP0vDQBiH3xJIlrc9xzuQfoabgoPUr3Kl0MmAkzjUUBBuqs6KX6IQKI6BYLOkuN4RB0FwcYkIpQ6Kr3+nBO0meM9w7487Hn73AjgcfxHvYyALxgBqbw1lU0xSUuQaZdvSKBq/UWTuXU4fLg5R2vt+dSNjusluKxj1gJ2PaxVx5A/tWZGjKKOEK5mBLIYhh/kA+HVaqzAPw7Kt59gpoykpKUgDIYBPgataxffYsnwmBewiWam3j5ngsYKXZoVa/LKlR7hh2jNq8UhByVu6WaFdQnusUxSTaLZFu6Aodvd5/2SA3NQr8iq7M0863mHBIrGrg7jbyfOkqpa9LjutVz7JvhO+n+orNBP/8O5wOBz/mlfwo1yu9LQ3OgAAAABJRU5ErkJggg==","orcid":"https://orcid.org/0000-0002-6612-903X","institution":"Shanghai Institute of Ceramics Chinese Academy of Sciences","correspondingAuthor":true,"submittingAuthor":false,"prefix":"","firstName":"Meng","middleName":"","lastName":"Xie","suffix":""},{"id":533372,"identity":"16518245-ffeb-44fd-8ebe-8f1707afb5a2","order_by":2,"name":"Yizheng Bao","email":"","orcid":"","institution":"Shanghai Institute of Materia Medica Chinese Academy of Sciences","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Yizheng","middleName":"","lastName":"Bao","suffix":""},{"id":533373,"identity":"cdbfc0d9-ae5f-449d-88c4-ebc3f121c1c0","order_by":3,"name":"Hengchang Nie","email":"","orcid":"","institution":"Shanghai Institute of Ceramics Chinese Academy of Sciences","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Hengchang","middleName":"","lastName":"Nie","suffix":""},{"id":533374,"identity":"f41702ce-1319-471e-8637-e2b8c7de540e","order_by":4,"name":"Fei Cao","email":"","orcid":"","institution":"Shanghai Institute of Ceramics Chinese Academy of Sciences","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Fei","middleName":"","lastName":"Cao","suffix":""},{"id":533375,"identity":"642ce8f0-c8d2-43d3-940d-3a392815f40f","order_by":5,"name":"Xianlin Dong","email":"","orcid":"","institution":"Shanghai Institute of Ceramics Chinese Academy of Sciences","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Xianlin","middleName":"","lastName":"Dong","suffix":""},{"id":533376,"identity":"5873f642-31dc-4ba5-9cc6-c4127da3ec0c","order_by":6,"name":"Genshui Wang","email":"","orcid":"","institution":"Shanghai Institute of Ceramics Chinese Academy of Sciences","correspondingAuthor":false,"submittingAuthor":false,"prefix":"","firstName":"Genshui","middleName":"","lastName":"Wang","suffix":""}],"badges":[],"createdAt":"2020-04-29 05:06:49","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-25916/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-25916/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":1037467,"identity":"62bb1006-6f56-487e-8655-41b97d56181a","added_by":"auto","created_at":"2020-05-06 14:05:00","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":2932498,"visible":true,"origin":"","legend":"X-ray diffraction patterns of PLZT ceramics with x = 0.01, 0.03, 0.04, 0.06, 0.07 in the range of (a) 10-80°, (b) 37-39°, (c) 43-45°.","description":"","filename":"Figure1.png","url":"https://assets-eu.researchsquare.com/files/rs-25916/v1/Figure1.png"},{"id":1037468,"identity":"1e258c6e-ca57-4fbd-ab00-9fbad4a6e9a1","added_by":"auto","created_at":"2020-05-06 14:05:00","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":3040114,"visible":true,"origin":"","legend":"Cross-sectional SEM microstructure of the PLZT ceramics with different La contents: (a) x = 0.01, (b) x = 0.03, (c) x = 0.04, (d) x = 0.06, (e) x = 0.07.","description":"","filename":"Figure2.png","url":"https://assets-eu.researchsquare.com/files/rs-25916/v1/Figure2.png"},{"id":1037469,"identity":"116b38e9-4b17-4106-9d52-d6d4a41e40de","added_by":"auto","created_at":"2020-05-06 14:05:00","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":5850181,"visible":true,"origin":"","legend":"Temperature-dependent relative dielectric constant (ε_r) and dielectric loss (tanδ) from room temperature to 350 ℃ for poled PLZT ceramics of (a) x = 0.01, (b) x = 0.03, (c) x = 0.04, (d) x = 0.06, (e) x = 0.07 at different frequencies. (f) Temperature-dependent relative dielectric constant (ε_r) and dielectric loss (tanδ) from room temperature to 350 ℃ for poled PLZT ceramics of (a) x = 0.01, (b) x = 0.03, (c) x = 0.04, (d) x = 0.06, (e) x = 0.07 at 10 kHz","description":"","filename":"Figure3.png","url":"https://assets-eu.researchsquare.com/files/rs-25916/v1/Figure3.png"},{"id":1037470,"identity":"a2153cb9-af14-49f4-ae2f-80212b157e47","added_by":"auto","created_at":"2020-05-06 14:05:00","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":7433602,"visible":true,"origin":"","legend":"Temperature-dependent P-E hysteresis loops of PLZT(x) under electric field of 4.0kV/mm (1 Hz), (f) Pr of PLZT(x) ceramics tested at different temperature under electric field of 4kV/mm (1 Hz)","description":"","filename":"Figure4.png","url":"https://assets-eu.researchsquare.com/files/rs-25916/v1/Figure4.png"},{"id":1037471,"identity":"32882613-7936-4981-ba0f-9bd94c715f61","added_by":"auto","created_at":"2020-05-06 14:05:00","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":5249257,"visible":true,"origin":"","legend":"P-E hysteresis loops (a1, b1) and current-field (I-E) curve (a2, b2) of polarized PLZT(x = 0.04, 0.06) ceramics at electric field of 4 kV/mm and under the hydrostatic pressure increasing from 0 MPa to 400 MPa","description":"","filename":"Figure5.png","url":"https://assets-eu.researchsquare.com/files/rs-25916/v1/Figure5.png"},{"id":1037472,"identity":"c40425d9-e437-4e21-af18-95406c770e9c","added_by":"auto","created_at":"2020-05-06 14:05:01","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":2932498,"visible":true,"origin":"","legend":"(a) The remnant polarization of PLZT (x = 0.04, 0.06) as function of hydrostatic pressure; (b) Phase diagram for poled (Pb1-1.5xLax)(Zr0.8Ti0.2)O3 ceramics of x = 0.01-0.07.","description":"","filename":"Figure6.png","url":"https://assets-eu.researchsquare.com/files/rs-25916/v1/Figure6.png"},{"id":15666837,"identity":"aec263be-9adb-40dc-b70b-8e3ee2e44f9f","added_by":"auto","created_at":"2021-11-18 13:38:59","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":4665699,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-25916/v1/d20f2d1c-0cfd-4ee4-8f06-18be725fb8a2.pdf"},{"id":1037466,"identity":"19f3051a-1874-4007-ba08-76712c9eedff","added_by":"auto","created_at":"2020-05-06 14:04:59","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"supplement","size":54662,"visible":true,"origin":"","legend":"","description":"","filename":"Equation1.pdf","url":"https://assets-eu.researchsquare.com/files/rs-25916/v1/Equation1.pdf"}],"financialInterests":"","formattedTitle":"\u003cp\u003eThe effects of composition, temperature and hydrostatic pressure on phase transition behaviors in (Pb\u003csub\u003e1-1.5x\u003c/sub\u003eLa\u003csub\u003ex\u003c/sub\u003e)(Zr\u003csub\u003e0.8\u003c/sub\u003eTi\u003csub\u003e0.2\u003c/sub\u003e)O\u003csub\u003e3 \u003c/sub\u003eceramics\u003c/p\u003e","fulltext":[{"header":"1. Introduction","content":" \u003cp\u003eFerroelectric (FE) lead-containing materials with spontaneous polarization, is the significant functional materials and has been studied for many years [1]. Lead zirconate titanate (Pb(Zr,Ti)O\u003csub\u003e3\u003c/sub\u003e, (PZT)) ceramics with outstanding piezoelectric and ferroelectric properties are representative compositional system for ferroelectric materials, widely utilized in modern ferroelectric transducers, sensor, actuators and ultrahigh-power system [2\u0026ndash;6].\u003c/p\u003e \u003cp\u003eBased on reported studies, modification with dopants has been an acknowledged and effective approach to optimize the performance of PZT ceramics [7\u0026ndash;12]. In particular, compositions near phase boundary have been concentrated on more interest over the past few decades, because of that phase transition of polar state and nonpolar state involving to the generation/release electric polarization have a wide range of applications [7, 13\u0026ndash;15]. Pb(Zr,Sn,Ti)O\u003csub\u003e3\u003c/sub\u003e, (Pb,Nb)(Zr,Sn,Ti)O\u003csub\u003e3\u003c/sub\u003e, and (Pb,La)(Zr,Sn,Ti)O\u003csub\u003e3\u003c/sub\u003e ceramics obtained through modification of PZT ceramics with Sn and La are all promising ferroelectric materials, extensively studied and applied [7, 8, 16].\u003c/p\u003e \u003cp\u003eIn addition, (Pb,La)(Zr,Ti)O\u003csub\u003e3\u003c/sub\u003e (PLZT) ceramics acquired through modification of PZT ceramics with lanthanum (La) are also representative ferroelectric materials [17\u0026ndash;22]. The coupling of ferroelectric reactive oxygen octahedrons broken by the replacement of La\u003csup\u003e3+\u003c/sup\u003e(1.36\u0026nbsp;\u0026Aring;) for Pb\u003csup\u003e2+\u003c/sup\u003e (1.49\u0026nbsp;\u0026Aring;) at A-sites give rise to phase transformation[19, 23]. In particular, the excellent piezoelectricity, pyroelectricity and energy-storage properties are possessed by compositions located in phased boundary [19, 24\u0026ndash;28]. For example, Ciuchi et al. investigated the energy storage performances of (Pb\u003csub\u003e1\u0026thinsp;\u0026minus;\u0026thinsp;\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003eLa\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e)(Zr\u003csub\u003e0.90\u003c/sub\u003eTi\u003csub\u003e0.10\u003c/sub\u003e)\u003csub\u003e1\u0026minus;\u003cem\u003ex\u003c/em\u003e/4\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e ceramics with La compositions near the FE-AFE phase boundary [26]. Qiao et al. reported the effect of FE-AFE phase transition on enhanced pyroelectric properties in (Pb\u003csub\u003e1\u0026thinsp;\u0026minus;\u0026thinsp;1.5\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003eLa\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e) (Zr\u003csub\u003e0.86\u003c/sub\u003eTi\u003csub\u003e0.14\u003c/sub\u003e) O\u003csub\u003e3\u003c/sub\u003e ceramics [27]. Besides, high piezoelectricity of PLZT ceramics near phase boundary was evident by Kumar et al [28]. In general, it\u0026rsquo;s fundamental and significant to investigate the phase transition in PLZT ceramics for application. However, to date, there were rare attentions paid to the effect of composition, temperature, especially, hydrostatic pressure on FE-AFE phase transition in (Pb\u003csub\u003e1\u0026thinsp;\u0026minus;\u0026thinsp;1.5\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003eLa\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e) (Zr\u003csub\u003e0.80\u003c/sub\u003eTi\u003csub\u003e0.20\u003c/sub\u003e) O\u003csub\u003e3\u003c/sub\u003e.\u003c/p\u003e \u003cp\u003eIn this paper, the effect of composition, temperature, and hydrostatic pressure on phase transition behaviors in (Pb\u003csub\u003e1\u0026thinsp;\u0026minus;\u0026thinsp;1.5\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003eLa\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e) (Zr\u003csub\u003e0.80\u003c/sub\u003eTi\u003csub\u003e0.20\u003c/sub\u003e)O\u003csub\u003e3\u003c/sub\u003e (\u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.01, 0.03, 0.04, 0.06, 0.07) ceramics are investigated thoroughly. XRD patterns, temperature-dependent \u003cem\u003eP-E\u003c/em\u003e hysteresis loops, and temperature-dependent dielectric constant curve demonstrate phase transition between FE\u003csub\u003eR\u003c/sub\u003e and AFE\u003csub\u003eT\u003c/sub\u003e driven by increased La content and temperature. What\u0026rsquo;s more, the depolarization behaviors of poled PLZT(\u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.04, 0.06) under hydrostatic pressure are investigated. These results indicate La doping at A-sites reconfigures the phase boundary of FE state and AFE state in PLZT ceramics. Besides, it also unveil the FE-AFE phase transition of (Pb\u003csub\u003e1\u0026thinsp;\u0026minus;\u0026thinsp;1.5\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003eLa\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e)(Zr\u003csub\u003e0.80\u003c/sub\u003eTi\u003csub\u003e0.20\u003c/sub\u003e)O\u003csub\u003e3\u003c/sub\u003e ceramics for promising potential engineering applications.\u003c/p\u003e "},{"header":"2. Experimental Procedure","content":" \u003cp\u003e(Pb\u003csub\u003e1\u0026thinsp;\u0026minus;\u0026thinsp;1.5\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003eLa\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e)(Zr\u003csub\u003e0.8\u003c/sub\u003eTi\u003csub\u003e0.2\u003c/sub\u003e)O\u003csub\u003e3\u003c/sub\u003e (\u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.01, 0.03, 0.04, 0.06, 0.07) ceramics were prepared via conventional solid reaction method. Raw materials were reagent-grade metal oxides Pb\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e (99.5%), La\u003csub\u003e2\u003c/sub\u003eO\u003csub\u003e3\u003c/sub\u003e (99.95%), ZrO\u003csub\u003e2\u003c/sub\u003e (99.99%), TiO\u003csub\u003e2\u003c/sub\u003e (99.21%). 0.5\u0026nbsp;mol% additional Pb\u003csub\u003e3\u003c/sub\u003eO\u003csub\u003e4\u003c/sub\u003e were added in order to compensate Pb volatilization during sintering. The powders were weighted according to the stoichiometric composition and ball milled 12\u0026nbsp;h in Teflon jars with deionized water and zirconium ball as media. After drying, the powders were calcined at 925\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e \\text{℃}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e for 2\u0026nbsp;h. And the calcined powders were ball milled again for 24\u0026nbsp;h. The polyvinyl alcohol (PVA), a binder for granulation, was mixed into calcined powders. The powders were pressed into pellets with 13\u0026nbsp;mm diameter. After burning off PVA, the pellets buried with same composition to minimize Pb volatilization in alumina crucible, were sintered at 1300 \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e \\text{℃}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e for 2\u0026nbsp;h with a heating rate of 2 \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e \\text{℃}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e/min. The sintered pellets were polished to a thickness of 0.5\u0026nbsp;mm and both sides of samples were covered with fired-on silver paste, calcined at 600\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e \\text{℃}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e for 2\u0026nbsp;h.\u003c/p\u003e \u003cp\u003eCrystal structure was studied by using X-ray diffraction (XRD, D/MAX-2550V; Rigaku, Tokyo, Japan). Cross-sectional microstructure was observed using a TM 3000 Tabletop Microscope (Hitachi, Tokyo, Japan). The dielectric constant (\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e {\\epsilon }_{r}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e) and tangent loss (\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e tan\\delta \u003c/script\u003e\u003c/span\u003e\u003c/span\u003e) were tested by using a LCR meter (Model E4980; Agilent, Palo Alto, CA, USA). Polarization-electric field (\u003cem\u003eP-E\u003c/em\u003e) hysteresis loops and depolarization behaviors under hydrostatic pressure were measured using an aixACCT TF 2000 Analyzer FE measuring by system (aix ACCT Co., Aachen, Germany) with home-made hydrostatic loading apparatus [29].\u003c/p\u003e "},{"header":"3. Result And Discussion","content":" \u003cdiv id=\"Sec4\" class=\"Section2\"\u003e \u003ch2\u003e3.1 Structure properties\u003c/h2\u003e \u003cp\u003eAs shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e, the perovskite structure with second phases PbO\u003csub\u003e2\u003c/sub\u003e (PDF#50-1430) is observed in the XRD patterns of PLZT ceramics. The peak is shifted slightly to higher 2\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e {\\theta }\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e with the increased La content, indicating decrease of lattice constant and smaller unit cell volume, attributed to oxygen octahedral distortion causing by the replacement of La\u003csup\u003e3+\u003c/sup\u003e(1.36\u0026nbsp;\u0026Aring;) for Pb\u003csup\u003e2+\u003c/sup\u003e (1.49\u0026nbsp;\u0026Aring;) at A-sites. Detailed XRD patterns in 2\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e {\\theta }\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e plotted in Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003eb and Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003ec, it can be observed the peak splitting in the (111) reflections in the PLZT ceramics of \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.01, 0.03, indicating a predominantly rhombohedral distortion, that is, the nature of FE\u003csub\u003eR\u003c/sub\u003e phase. With increased La content (\u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.04, 0.06, 0.07), the peak splitting are observed in the (200) reflections and the (111) reflections are gradually transformed to single peak, indicating the phase switching to tetragonal distortion, that is, the coexistence of FE\u003csub\u003eR\u003c/sub\u003e phase and AFE\u003csub\u003eT\u003c/sub\u003e phase [30]. The result reveals that the occurrence of FE\u003csub\u003eR\u003c/sub\u003e-AFE\u003csub\u003eT\u003c/sub\u003e phase transition is driven by increased La content.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe cross-sectional SEM images of fresh samples sintered at 1300\u0026nbsp;\u0026deg;C are shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e. With increased La content, the grain size is decreased significantly. In addition, these cross-sections are fractured along intergranular direction under external force when La content \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.01, 0.03 and 0.04; whereas cross-sections for \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.06 and 0.07 are fractured along trans-granular direction under external force.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section2\"\u003e \u003ch2\u003e3.2 Dielectric properties\u003c/h2\u003e \u003cp\u003eTemperature-dependent relative dielectric constant (\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e {\\epsilon }_{r}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e) and dielectric loss (\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e tan\\delta \u003c/script\u003e\u003c/span\u003e\u003c/span\u003e) of PLZT ceramics as a function of temperature at different frequencies are displayed in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ea-e. Similar temperature-dependent behavior at the Curie temperature\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e {(T}_{C})\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e are obsevered in the samples of \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.01 and 0.03. \u003cem\u003eT\u003c/em\u003e\u003csub\u003eC\u003c/sub\u003e is defined by the temperature of the maximum dielectric constent, regarded as a thermodynamic scale for the transition energy barrier from the FE or AFE phase to paraelectric (PE) phase. [31] While two dielectric anomalies can be observed in the PLZT ceramics of \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.04 and 0.06: \u003cem\u003eT\u003c/em\u003e\u003csub\u003eFE\u0026minus;AFE\u003c/sub\u003e and \u003cem\u003eT\u003c/em\u003e\u003csub\u003eC\u003c/sub\u003e. \u003cem\u003eT\u003c/em\u003e\u003csub\u003eFE\u0026minus;AFE\u003c/sub\u003e can be determined by the first dielectric constant inflection point and dielectric loss peak, attributed to the transformation from FE to AFE. Hence, \u003cem\u003eT\u003c/em\u003e\u003csub\u003eFE\u0026minus;AFE\u003c/sub\u003e has also been regared as the depolarization temperature (\u003cem\u003eT\u003c/em\u003e\u003csub\u003e\u003cem\u003ed\u003c/em\u003e\u003c/sub\u003e) of the sample. As for the sample with \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.07, it can be only seen phase transition from AFE to PE since the AFE phase is dominanted. In Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ef, the \u003cem\u003eT\u003c/em\u003e\u003csub\u003e\u003cem\u003eC\u003c/em\u003e\u003c/sub\u003e corresponding to the samples of \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.01, 0.03, 0.04, 0.06, 0.07 are 240\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e \\text{℃}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e, 207\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e \\text{℃}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e, 143\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e \\text{℃}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e, 128\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e \\text{℃}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e, 114\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e \\text{℃}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e, respectively. Furthermore, \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e \\epsilon \u003c/script\u003e\u003c/span\u003e\u003c/span\u003e\u003csub\u003emax\u003c/sub\u003e is decreased from 42025 to 5435 with increased La content, and the \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e tan\\delta \u003c/script\u003e\u003c/span\u003e\u003c/span\u003e is less than 0.083. Therefore, it is confirmed that the PLZT ceramics of \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.04, 0.06 are lying around the FE-AFE phase boundaries and experience FE-AFE phase transition near 125\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e \\text{℃}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e and 80\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e \\text{℃}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e, while the PLZT ceramics of \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.01, 0.03 are stable FE\u003csub\u003eR\u003c/sub\u003e before \u003cem\u003eT\u003c/em\u003e\u003csub\u003e\u003cem\u003eC\u003c/em\u003e\u003c/sub\u003e.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec6\" class=\"Section2\"\u003e \u003ch2\u003e3.3 Ferroelectric properties\u003c/h2\u003e \u003cp\u003eThe \u003cem\u003eP-E\u003c/em\u003e hysteresis loops of all as-sintered specimens from 30\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e \\text{℃}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e to 170\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e \\text{℃}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e can be observed in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e to further confirmed temperature-induced phase transition shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e. As shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ea, b, well-shaped \u003cem\u003eP-E\u003c/em\u003e hysteresis loops show that these components are stable FE\u003csub\u003eR\u003c/sub\u003e independent of temperature, where 170\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e \\text{℃}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e is less than \u003cem\u003eT\u003c/em\u003e\u003csub\u003eC\u003c/sub\u003e shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ea and b. PLZT ceramics of \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.04, 0.06 are transformed from well-shaped \u003cem\u003eP-E\u003c/em\u003e loops to double hysteresis loops and then to slim P-E loops, indicating transition of FE phase to AFE phase and then to PE phase [32, 33]. Phase transformation from AFE to PE with La content \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.07 is exhibited in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ee. Moreover, the phase transition temperature is decreased from about 130 \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e \\text{℃}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e to 90 \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e \\text{℃}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e with increased La content corresponding to Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ef, in which defects produced by the aliovalent substitution and the long range order of ferroelectric domains destroyed are beneficial to the inversion of domain wall [34]. \u003cem\u003eP\u003c/em\u003e\u003csub\u003e\u003cem\u003er\u003c/em\u003e\u003c/sub\u003e and coercive field \u003cem\u003eE\u003c/em\u003e\u003csub\u003e\u003cem\u003eC\u003c/em\u003e\u003c/sub\u003e are decreased remarkably and the loops are much slimmer with further increased temperature and La content [1]. In the Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ef and Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003ef, it can be observed excellent temperature stability for \u003cem\u003eP\u003c/em\u003e\u003csub\u003e\u003cem\u003er\u003c/em\u003e\u003c/sub\u003e of samples of \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.01, 0.03; while there is a sharp decrease in \u003cem\u003eP\u003c/em\u003e\u003csub\u003e\u003cem\u003er\u003c/em\u003e\u003c/sub\u003e for samples of \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.04, 0.06, proving temperature dominates FE-AFE transition. In a way, there is temperature-induced structural phase transition and depolarization behaviors in the PLZT ceramics of \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.04 and 0.06.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec7\" class=\"Section2\"\u003e \u003ch2\u003e3.4 Depolarization under hydrostatic pressure\u003c/h2\u003e \u003cp\u003ePLZT(\u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.04, 0.06) ceramics with higher \u003cem\u003eP\u003c/em\u003e\u003csub\u003e\u003cem\u003er\u003c/em\u003e\u003c/sub\u003e and near the phase boundary between FE and AFE phase are chosen to study the depolarization under hydrostatic pressure. These samples were polarized at 2.0\u0026nbsp;kV/mm for 15\u0026nbsp;min at room temperature in an silicone oil bath, and then placed for 24\u0026nbsp;h after polarization to obtain stable \u003cem\u003eP\u003c/em\u003e\u003csub\u003e\u003cem\u003er\u003c/em\u003e\u003c/sub\u003e. \u003cem\u003eP-E\u003c/em\u003e hysteresis loops and \u003cem\u003eI-E\u003c/em\u003e loops of PLZT(\u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.04, 0.06) ceramics at electric field of 4\u0026nbsp;kV/mm and under the hydrostatic pressure increasing from 0\u0026nbsp;MPa to 400\u0026nbsp;MPa are shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e. Well-shaped P-E hysteresis loops with the \u003cem\u003eP\u003c/em\u003e\u003csub\u003e\u003cem\u003er\u003c/em\u003e\u003c/sub\u003e decreased from 29.11 \u0026micro;C/cm\u003csup\u003e2\u003c/sup\u003e to 19.76 \u0026micro;C/cm\u003csup\u003e2\u003c/sup\u003e are shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e(a1). It\u0026rsquo;s also observed that the maximum pressure used in the experiment do not reach the critical depolarization pressure. What\u0026rsquo;s more, \u003cem\u003eE\u003c/em\u003e\u003csub\u003e\u003cem\u003eC\u003c/em\u003e\u003c/sub\u003e is decreased from 1.09 to 0.94\u0026nbsp;kV/mm with increased pressure to 400\u0026nbsp;MPa, indicating that a predominant FE ordering gradually decreases. As shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e\u003cb\u003e(\u003c/b\u003ea2), with increased hydrostatic pressure, the current peak gradually slows down and the polarization is gradually released in the form of current under additional field. Clearly, the \u003cem\u003eP\u003c/em\u003e\u003csub\u003e\u003cem\u003er\u003c/em\u003e\u003c/sub\u003e of sample \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.06 is decreased from 31.52 \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e {\\mu }\u003c/script\u003e\u003c/span\u003e\u003c/span\u003eC/cm\u003csup\u003e2\u003c/sup\u003e to 6.45 \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e {\\mu }\u003c/script\u003e\u003c/span\u003e\u003c/span\u003eC/cm\u003csup\u003e2\u003c/sup\u003e, as shown in the Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e(b1). It\u0026rsquo;s exhibited in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e\u003cb\u003e(\u003c/b\u003eb2) that the single current peak is transformed to double current peak with the transition from FE\u003csub\u003eR\u003c/sub\u003e phase to AFE\u003csub\u003eT\u003c/sub\u003e phase under the effect of hydrostatic pressure, which is similar to temperature-induced phase transition shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e and Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e. According to soft mode theory, hydrostatic pressure with spherical symmetry increases the interactions between adjacent cations and anions more rapidly than it increases long-range Coulomb forces, increasing the AFE phase stability, and releasing stored charges in a very short period of time [30].\u003c/p\u003e \u003cp\u003eTo further evaluate pressure-induced depolarization behaviors, the remnant polarization of poled PLZT (\u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.04, 0.06) are shown in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e(a). It can be observed that the \u003cem\u003eP\u003c/em\u003e\u003csub\u003e\u003cem\u003er\u003c/em\u003e\u003c/sub\u003e of \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.04 is decreased steadily under hydrostatic pressure, and the \u003cem\u003eP\u003c/em\u003e\u003csub\u003e\u003cem\u003er\u003c/em\u003e\u003c/sub\u003e of \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.06 is decreased rapidly after hydrostatic pressure of 250\u0026nbsp;MPa. Meanwhile, the remnant polarizations are decreased from \u003cem\u003eP\u003c/em\u003e\u003csub\u003e\u003cem\u003er1\u003c/em\u003e\u003c/sub\u003e = 29.11 \u0026micro;C/cm\u003csup\u003e2\u003c/sup\u003e, 31.52 \u0026micro;C/cm\u003csup\u003e2\u003c/sup\u003e to \u003cem\u003eP\u003c/em\u003e\u003csub\u003e\u003cem\u003er2\u003c/em\u003e\u003c/sub\u003e = 19.76 \u0026micro;C/cm\u003csup\u003e2\u003c/sup\u003e, 6.45 \u0026micro;C/cm\u003csup\u003e2\u003c/sup\u003e, respectively, with depolarization rates of 32.12% and 79.54%,calculated by (see Equation 1 in the Supplementary Files) \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e {R}_{T}=-\\frac{{P}_{r2}-{P}_{r1}}{{P}_{r1}}\\times 100\\%\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e under 400\u0026nbsp;MPa pressure. These results demonstrate that the oriented FE domains are rearranged under the influence of hydrostatic pressure, accompanied by irreversible FE-AFE phase transition and the release of polarization. The results also demonstrate the promising potential application of (Pb\u003csub\u003e1\u0026minus;1.5\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003eLa\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e)(Zr\u003csub\u003e0.8\u003c/sub\u003eTi\u003csub\u003e0.2\u003c/sub\u003e)O\u003csub\u003e3\u003c/sub\u003e ceramics in pulsed power supply.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eBased on the above results, a simple phase diagram of (Pb\u003csub\u003e1\u0026thinsp;\u0026minus;\u0026thinsp;1.5\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003eLa\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e)(Zr\u003csub\u003e0.8\u003c/sub\u003eTi\u003csub\u003e0.2\u003c/sub\u003e)O\u003csub\u003e3\u003c/sub\u003e ceramics is proposed. The phase diagram of PLZT ceramics for \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.01, 0.03, 0.04, 0.06, 0.07 are summarized in Fig.\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e(b), determined by the temperature of \u003cem\u003eT\u003c/em\u003e\u003csub\u003e\u003cem\u003eC\u003c/em\u003e\u003c/sub\u003e corresponding to the maximum values of dielectric constant and dielectric loss in the Fig.\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e, employed to classify the boundary of FE and PE phase. The AFE phase can be stabilized by doping La\u003csup\u003e3+\u003c/sup\u003e and destabilized by Ti\u003csup\u003e4+\u003c/sup\u003e doping [5], so that PLZT ceramics are transformed from FE to AFE phase with La doping, manifesting AFE phase tends to be stable and a FE-AFE phase boundary is constructed by La in PLZT-based ceramics [35, 36].\u003c/p\u003e \u003c/div\u003e "},{"header":"4. Conclusion","content":" \u003cp\u003eIn summary, the effect of composition, temperature and hydrostatic pressure on phase transition behaviors in (Pb\u003csub\u003e1\u0026thinsp;\u0026minus;\u0026thinsp;1.5\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003eLa\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e)(Zr\u003csub\u003e0.80\u003c/sub\u003eTi\u003csub\u003e0.20\u003c/sub\u003e)O\u003csub\u003e3\u003c/sub\u003e ceramics were investigated thoroughly, with emphasis on ferroelectric, dielectric performances, and depolarization behaviors. With increased La content, PLZT (\u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.01, 0.03, 0.04, 0.06, 0.07) ceramics underwent transition from FE\u003csub\u003eR\u003c/sub\u003e phase to AFE\u003csub\u003eT\u003c/sub\u003e phase. Aliovalent A-site substitution of La\u003csup\u003e3+\u003c/sup\u003e doping interrupted long-range ordered ferroelectric domains, driving FE\u003csub\u003eR\u003c/sub\u003e-AFE\u003csub\u003eT\u003c/sub\u003e phase switching. The lattice constant was decreased and the peak value was shifted to higher 2\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e {\\theta }\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e as a whole. Temperature-dependent P-E hysteresis loops and temperature-dependent relative dielectric constant (\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e {\\epsilon }_{r}\u003c/script\u003e\u003c/span\u003e\u003c/span\u003e) and dielectric loss (\u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\u003cscript type=\"math/tex; mode=inline\"\u003e tan\\delta \u003c/script\u003e\u003c/span\u003e\u003c/span\u003e) demonstrated PLZT(\u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.01, 0.03) ceramics were stable FE\u003csub\u003eR\u003c/sub\u003e phase, while PLZT(\u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.04, 0.06, 0.07) coexisted FE phase and AFE phase. With the increase of temperature, the domains overcame the energy barrier to achieve FE-AFE phase transition. There was thermal-induced FE-AFE phase transition and depolarization behaviors in the PLZT ceramics of \u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.04, 0.06. Pressure-dependent P-E loops and I-E loops illustrated the polarized sample PLZT (\u003cem\u003ex\u003c/em\u003e\u0026thinsp;=\u0026thinsp;0.04, 0.06) ceramic could be depolarized with depolarization rate of 38.51% and 79.54%, respectively. According to the effect of external field on FE-AFE phase transition, it indicated that (Pb\u003csub\u003e1\u0026thinsp;\u0026minus;\u0026thinsp;1.5\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003eLa\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e)(Zr\u003csub\u003e0.8\u003c/sub\u003eTi\u003csub\u003e0.2\u003c/sub\u003e)O\u003csub\u003e3\u003c/sub\u003e ceramics had promising potential in the field engineering application.\u003c/p\u003e "},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eAcknowledgements \u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThis work was supported by National Natural Science Foundation of China (Grant No. 11774366, 51872312), Youth Innovation Promotion Association, CAS (Grant No. 2017296), and Natural Science Foundation of Shanghai (Grant NO.18ZR1444900).\u003c/p\u003e"},{"header":"References","content":"\u003cp\u003e[1] Haertling G H. 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Thermal-induced structural transition and depolarization behavior in (Bi\u003csub\u003e0.5\u003c/sub\u003eNa\u003csub\u003e0.5\u003c/sub\u003e)TiO\u003csub\u003e3\u003c/sub\u003e-BiAlO\u003csub\u003e3\u003c/sub\u003e ceramics. \u003cem\u003eJ Appl Phys\u003c/em\u003e 2018, \u003cstrong\u003e123\u003c/strong\u003e: 114102.\u003c/p\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":true,"highlight":"","institution":"","isAcceptedByJournal":false,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true},"keywords":"Phase transition, PLZT, ferroelectrics, anti-ferroelectrics","lastPublishedDoi":"10.21203/rs.3.rs-25916/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-25916/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eIn this work, (Pb\u003csub\u003e1 − 1.5\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003eLa\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e)(Zr\u003csub\u003e0.80\u003c/sub\u003eTi\u003csub\u003e0.20\u003c/sub\u003e)O\u003csub\u003e3\u003c/sub\u003e (abbreviated as PLZT, \u003cem\u003ex\u003c/em\u003e = 0.01, 0.03, 0.04, 0.06, 0.07) ceramics are designed on the base of chemical composition modification and prepared by solid-state reaction. The effect of composition, temperature, and hydrostatic pressure on ferroelectric-antiferroelectric (FE-AFE) phase transition is investigated. It is obtained that phase transition from ferroelectric rhombohedral phase to antiferroelectric tetragonal phase as a function of La\u003csup\u003e3+\u003c/sup\u003e doping content, especially, the PLZT ceramics of \u003cem\u003ex\u003c/em\u003e = 0.04, 0.06, and 0.07 are the coexistence of FE-AFE phase. It is also found the FE-AFE phase transition driven by increased temperature in poled PLZT ceramics (\u003cem\u003ex\u003c/em\u003e = 0.04, 0.06). Furthermore, static charges density (\u003cem\u003eP\u003c/em\u003e\u003csub\u003e\u003cem\u003er\u003c/em\u003e\u003c/sub\u003e) of PLZT (\u003cem\u003ex\u003c/em\u003e = 0.04, 0.06) are decreased from 29.11 µC/cm\u003csup\u003e2\u003c/sup\u003e and 31.52 µC/cm\u003csup\u003e2\u003c/sup\u003e to 19.76 {\\mu }C/cm\u003csup\u003e2\u003c/sup\u003e, 6.45 {\\mu }C/cm\u003csup\u003e2\u003c/sup\u003e under 400\u0026nbsp;MPa hydrostatic pressure due to the pressure-induced FE-AFE phase transition. The depolarization rates are 32.12% and 79.54%, respectively. Meanwhile, the phase diagram of (Pb\u003csub\u003e1 − 1.5\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003eLa\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e)(Zr\u003csub\u003e0.80\u003c/sub\u003eTi\u003csub\u003e0.20\u003c/sub\u003e)O\u003csub\u003e3\u003c/sub\u003e ceramics is acquired roughly. These results provide guidance for the engineering application of (Pb\u003csub\u003e1 − 1.5\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003eLa\u003csub\u003e\u003cem\u003ex\u003c/em\u003e\u003c/sub\u003e)(Zr\u003csub\u003e0.80\u003c/sub\u003eTi\u003csub\u003e0.20\u003c/sub\u003e)O\u003csub\u003e3\u003c/sub\u003e ceramics.\u003c/p\u003e","manuscriptTitle":"The effects of composition, temperature and hydrostatic pressure on phase transition behaviors in (Pb1-1.5xLax)(Zr0.8Ti0.2)O3 ceramics","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2020-05-06 14:04:59","doi":"10.21203/rs.3.rs-25916/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"de9ce8a1-7dd1-4501-8a51-60cd0b8ec9b2","owner":[],"postedDate":"May 6th, 2020","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[{"id":94540,"name":"Ceramics"}],"tags":[],"updatedAt":"2020-05-29T02:56:15+00:00","versionOfRecord":[],"versionCreatedAt":"2020-05-06 14:04:59","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-25916","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-25916","identity":"rs-25916","version":["v1"]},"buildId":"7rjqhiLT3MXkJMwkYKINL","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}